牛奶中苯并咪唑类药物及其代谢物残留的UPLC-MS/MS检测方法研究

建立了牛奶中苯并咪唑类药物及代谢物残留的UPLC-MS/MS检测方法。牛奶样品在弱碱性条件下经乙腈沉淀蛋白后,用乙酸乙酯提取,再经正己烷脱脂,MCX固相萃取柱净化,采用UPLC-MS/MS多反应监测(MRM)模式检测,外标法定量。本方法对苯并咪唑类药物及代谢物的检测限均为5μg/g,定量限均为10μg/g,在10～200μg/L添加浓度范围内回收率为69.9%～113.1%之间,批内变异系数在1.36%～11.48%之间,批间变异系数在1.09%～9.87%之间。本方法分析速度快,灵敏度高,重现性好,各项技术指标均满足国内外相关法规要求,可用于牛奶中苯并咪唑类药物及代谢物残留的检测。

Determination of benzimidazoles and its metabolites residues in milk by ultra performance liquid chromatography- tandem mass spectrometry

A method based on UPLC-MS/MS has been developed for the determination of benzimidazoles and its metabolites residues in milk.The samples were precipitated by acetonitrile,and the analytes were extracted with ethyl acetate.Then the extract was cleaned by MCX solid phase extraction cartridge.Quantification of all the analytes was achieved by UPLC-MS/MS with multiple reaction monitoring（MRM） using external standard method.Detection limits and quantification limits of this method for the analysis were all 5 and 10 μg/g.The overall recovery varies from 69.9%～113.1% at the spiked level of 10～200 μg/L,and the intra-and inter-batch coefficients was from 1.36%～11.48% and from 1.09%～9.87%,respectively.The method was reliable,sensitive and reproducibility,its performance can meet the requirements of the domestic and international legislation.The method adapts to the determination of benzimidazoles and its metabolites residues in milk.